HPLC法测定中兽药散剂中非法添加土霉素的方法研究

Study on the Determination Method of Oxytetracycline Added Illegally in Veterinary Chinese Materia Medica Powders by HPLC

建立了高效液相色谱法检测清肺散、白头翁散、止痢散等中兽药散剂中非法添加土霉素的方法。用十八烷基硅烷键合硅胶色谱柱,以0.05 mol/L草酸铵溶液-二甲基甲酰胺-0.2 mol/L磷酸氢二铵(75∶20∶5)(用氨试液调pH值至8.0±0.2)为流动相,检测波长280 nm,流速1.0mL/min,进样量20μL,柱温35℃。结果显示,土霉素的线性范围为100～300μg/mL,线性方程为Y=4.90×10 X-2.39×103(,r=0.999 6,n=5),本方法的回收率为80.68%～119.23%,RSD为0.66%～1.85%。结果表明,本方法准确、可靠,适用于中兽药散剂中非法添加土霉素的检测。

An HPLC method was established for effective detection on oxytetracycline added illegally in veterinary Chinese materia medica powders as Qingfei San,Baitouweng San and Zhili San,etc.A reverse-phase C18 column was used,the mobile phase was 0.05 mol/L ammonium oxalate solution-DMF-0.2 mol/L ammonium dibasic phosphate（75∶ 20∶ 5）（adjusted the pH value with ammoniac solution to 8.0±0.2）,the determination wave length was 280 nm,the flow rate was 1.0 mL/min and the column worked at 35 ℃.The result demonstrated that the linearity range of oxytetracycline was 100~300 μg/mL,the linear equation is Y=4.90×10 X-2.39×103（r=0.999 6,n=5）,the recovery was 80.68%~119.23%,RSD was 0.66%~1.85%.It indicated that this method was accurate,reliable,and suitable in the determination of oxytetracycline added illegally in veterinary Chinese materia medica powders.